CN117865659A - Preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic - Google Patents
Preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 101
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 101
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 61
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000005350 fused silica glass Substances 0.000 title claims abstract description 44
- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000015895 biscuits Nutrition 0.000 claims abstract description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004327 boric acid Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 6
- 239000010440 gypsum Substances 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract 2
- 239000002002 slurry Substances 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 9
- 239000010453 quartz Substances 0.000 abstract description 5
- 239000011268 mixed slurry Substances 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000005452 bending Methods 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 3
- 239000011153 ceramic matrix composite Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
- C04B35/62857—Coating fibres with non-oxide ceramics
- C04B35/62865—Nitrides
- C04B35/62868—Boron nitride
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention discloses a preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic, which comprises the following steps: firstly, chopping and immersing carbon fibers into a precursor solution of boric acid dissolved in methanol, introducing ammonia gas into the boronized short carbon fibers under the condition of nitrogen gas, and heating to obtain boron nitride modified short carbon fibers; adding the boron nitride modified short carbon fiber, the fused quartz powder and the pure water into a ball mill for mixed ball milling; adding the mixed slurry into a gypsum mold for molding; and (5) placing the molded biscuit into a drying oven for drying, and finally placing the biscuit into a muffle furnace for sintering to obtain the boron nitride modified short carbon fiber reinforced fused quartz ceramic. The method has simple process, and the prepared quartz ceramic composite material has good mechanical property and low heat conductivity coefficient, and is suitable for industrial production.
Description
Technical Field
The invention relates to preparation of a quartz ceramic matrix composite material, in particular to a preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic.
Background
Ceramics and ceramic composite materials are very promising materials due to their high strength, high modulus, high hardness, high temperature resistance, corrosion resistance, and the like. However, ceramics have very low fracture toughness and high brittleness, which limits their use to some extent.
In the field of space-saving structural materials, carbon fiber reinforced ceramic matrix composites exhibit a wide range of properties including high strength, high stiffness, excellent toughness, low density, unique wear resistance, environmental stability, and the like, and particularly fused silica ceramics have very strong corrosion and thermal shock resistance, low coefficient of thermal expansion and low and stable dielectric constants, and very low mass loss rates at high temperatures. These properties indicate that carbon fiber reinforced fused silica composites are good radome candidates.
The patent with publication number CN103482994A discloses a preparation method of a carbon fiber reinforced quartz ceramic matrix composite material, but the method has the advantages of high carbon fiber content, poor toughening effect and complex process, and is not suitable for industrialization; the patent with publication number CN110194674A discloses a preparation method of a carbon fiber toughened quartz ceramic matrix composite material, and the tensile strength and the bending strength of the composite material prepared by the method are still low, and the toughening effect is not obvious.
Disclosure of Invention
The invention aims to provide a preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic, which has simple process, and the prepared quartz ceramic composite material has good mechanical property and low heat conductivity coefficient and is suitable for industrial production.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic comprises the following steps:
(1) Boron nitride modified short carbon fibers;
firstly, chopping carbon fibers to obtain short carbon fibers, then placing the short carbon fibers in acetone for soaking, then washing with distilled water and drying;
dissolving boric acid in pure methanol to obtain a precursor solution, completely immersing the short carbon fiber obtained in the step (1-1) in the precursor solution, ultrasonically stirring, separating the treated short carbon fiber from the solution, and drying in an oven;
(1-3) placing the boronized short carbon fibers obtained in the step (1-2) into a zirconia crucible, installing the crucible in a heating pipe, introducing ammonia gas under nitrogen condition, and heating to obtain boron nitride modified short carbon fibers;
(2) Adding the boron nitride modified short carbon fiber, fused quartz powder and pure water obtained in the step (1) into a ball mill for mixing and ball milling to obtain slurry;
(3) Adding the slurry mixed in the step (2) into a gypsum mold to form a biscuit;
(4) And (3) placing the biscuit obtained in the step (3) into an oven for drying, and finally placing the biscuit into a muffle furnace for sintering to obtain the boron nitride modified short carbon fiber reinforced fused quartz ceramic.
Preferably, in the step (2), the addition amount of the boron nitride modified short carbon fiber is 5wt.% to 20wt.% of the slurry; the addition amount of the fused quartz powder is 70-80 wt.% of the slurry; the addition amount of the pure water is 10wt.% to 15wt.% of the slurry.
Preferably, in the step (2), the rotating speed of the ball mill is 15-30r/min, and the ball milling time is 12-24h.
Preferably, in the step (4), the drying environment of the biscuit is: drying in an oven at 80-120 ℃ for 12-24 h; the specific system of sintering is as follows: and (3) placing the dried biscuit in a muffle furnace, heating to 1150-1250 ℃ from room temperature at a speed of 15 ℃/min under the air condition, and preserving heat for 3-5 hours to obtain the boron nitride modified short carbon fiber reinforced fused silica ceramic.
Preferably, in the step (1-3), the specific heating process by introducing ammonia gas is as follows: introducing ammonia gas at a speed of 10-50cc/min under the nitrogen condition, heating to 1400 ℃, preserving heat for 60-120min, stopping flowing of the ammonia gas after 1-2h, and cooling under the nitrogen atmosphere to obtain the boron nitride modified short carbon fiber.
Preferably, in the step (1-2), the mass ratio between boric acid and methanol is 1 (1-3); stirring by ultrasonic for 40-60min; the drying temperature of the oven is 60-100 ℃.
Preferably, in the step (1-1), the length of the short carbon fiber is 3-5cm; soaking short carbon fiber in acetone for 12-24 hr, washing with distilled water for 3-5 times, and drying in oven at 60-100deg.C for 12-24 hr.
Compared with the prior art, the invention has the following beneficial effects:
1. the boron nitride modified short carbon fiber has the advantages of low boron nitride heat conductivity coefficient, large mechanical load transfer, good high-temperature stability, light weight, capability of enhancing the interfacial adhesion between matrixes and excellent dielectric property.
2. The boron nitride modified short carbon fiber can obviously improve the ablation resistance of the composite material, and has obvious effect of improving the mechanical property of the composite material; the prepared boron nitride modified short carbon fiber reinforced fused quartz ceramic has high strength, low thermal conductivity and good dielectric property, and is an ideal radome material.
3. The method has the advantages of low equipment cost, few production procedures, high efficiency and unique advantages in the aspect of producing the special-shaped large-size ceramic.
Drawings
FIG. 1 is a transmission electron micrograph of a boron nitride modified short carbon fiber reinforced fused silica ceramic prepared in example 2 of the present invention.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
Example 1
A preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic comprises the following steps:
(1) Boron nitride modified short carbon fibers;
cutting the carbon fiber to 3-5cm, soaking the short carbon fiber in acetone for 12h, washing with distilled water for 3 times, and drying in an oven at 60 ℃ for 24h;
dissolving boric acid in pure methanol to obtain a precursor solution, wherein the mass ratio of the boric acid to the methanol is 1:1, immersing the short carbon fiber obtained in the step (1-1) in the precursor solution, ultrasonically stirring for 60min, separating the treated short carbon fiber from the solution, and putting the solution into a baking oven at 60 ℃ until the short carbon fiber is completely dried;
(1-3) placing the boronated short carbon fiber obtained in step (1-2) into a zirconia crucible and installing in a heating pipe; introducing ammonia gas at a speed of 10cc/min under the condition of nitrogen, heating to 1400 ℃, preserving heat for 120min, stopping flowing of the ammonia gas after 2h, and cooling under the atmosphere of nitrogen to obtain boron nitride modified short carbon fibers;
(2) Adding the boron nitride modified short carbon fiber, the fused quartz powder and the pure water prepared in the step (1) into a roller ball mill for mixed ball milling to obtain slurry; the adding amount of the boron nitride modified short carbon fiber is 5wt% of the slurry; the addition amount of the fused quartz powder is 80wt% of the slurry; the addition amount of pure water is 15wt% of the slurry; the rotating speed of the ball mill is 15r/min, and the ball milling time is 12h;
(3) Adding the mixed slurry obtained in the step (2) into a gypsum mold for molding;
(4) And (3) placing the biscuit molded in the step (3) into an oven with the temperature of 80 ℃ for drying for 24 hours, finally placing the biscuit into a muffle furnace, heating to 1150 ℃ from room temperature at the speed of 15 ℃/min under the air condition, and preserving heat for 5 hours to obtain boron nitride modified short carbon fiber reinforced fused silica ceramic, and respectively testing the dielectric constant, the thermal conductivity and the bending strength of the ceramic, wherein the testing standard or method and the obtained performance parameters are shown in the following table 1.
TABLE 1 boron nitride modified short carbon fiber reinforced fused silica ceramic Performance test results
Performance of | Test standard/method | Performance parameters |
Dielectric constant | Short circuit waveguide method | 3.5 |
Thermal conductivity (W/m.K) | Laser pulse method | <0.55 |
Flexural Strength (MPa) | GB/T 6569-2006 | 153 |
Example 2
A preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic comprises the following steps:
(1) Boron nitride modified short carbon fibers;
cutting the carbon fiber to 3-5cm, soaking the short carbon fiber in acetone for 18h, washing with distilled water for 4 times, and drying in an oven at 80 ℃ for 18h;
dissolving boric acid in pure methanol to obtain a precursor solution, wherein the mass ratio of the boric acid to the methanol is 1:2, immersing the short carbon fiber obtained in the step (1-1) in the precursor solution, ultrasonically stirring for 40min, separating the treated short carbon fiber from the solution, and putting the solution into an oven at 80 ℃ until the short carbon fiber is completely dried;
(1-3) placing the boronated short carbon fiber obtained in step (1-2) into a zirconia crucible and installing in a heating pipe; introducing ammonia gas at 30cc/min under the condition of nitrogen, heating to 1400 ℃, preserving heat for 80min, stopping flowing of the ammonia gas after 1.5h, and cooling under the atmosphere of nitrogen to obtain boron nitride modified short carbon fibers;
(2) Adding the boron nitride modified short carbon fiber, the fused quartz powder and the pure water prepared in the step (1) into a roller ball mill for mixed ball milling to obtain slurry; the adding amount of the boron nitride modified short carbon fiber is 15wt% of the slurry; the addition amount of the fused quartz powder is 75wt% of the slurry; the addition amount of the pure water is 10wt% of the slurry; the rotating speed of the ball mill is 20r/min, and the ball milling time is 18h:
(3) Adding the mixed slurry obtained in the step (2) into a gypsum mold for molding;
(4) And (3) placing the biscuit molded in the step (3) into an oven with the temperature of 100 ℃ to be dried for 18 hours, finally placing the biscuit into a muffle furnace, heating to 1200 ℃ from room temperature at the speed of 15 ℃/min under the air condition, and preserving heat for 4 hours to obtain boron nitride modified short carbon fiber reinforced fused silica ceramic, and respectively testing the dielectric constant, the thermal conductivity and the bending strength of the ceramic, wherein the testing standard or method and the obtained performance parameters are shown in the following table 2.
TABLE 2 Performance test results of boron nitride modified short carbon fiber reinforced fused silica ceramics
Performance of | Test standard/method | Performance parameters |
Dielectric constant | Short circuit waveguide method | 3.4 |
Thermal conductivity (W/m.K) | Laser pulse method | <0.59 |
Flexural Strength (MPa) | GB/T 6569-2006 | 161 |
Fig. 1 is a transmission electron micrograph of a boron nitride modified short carbon fiber reinforced fused silica ceramic prepared in an embodiment, and it can be seen from the figure that in the boron nitride modified short carbon fiber material, boron nitride is successfully and uniformly and tightly attached to the short carbon fiber, which is beneficial to reducing the thermal conductivity coefficient of the composite material and increasing the high-temperature stability of the composite material.
Example 3
A preparation method of boron nitride modified short carbon fiber reinforced fused quartz ceramic comprises the following steps:
(1) Boron nitride modified short carbon fibers;
cutting the carbon fiber to 3-5cm, soaking the short carbon fiber in acetone for 24h, washing with distilled water for 5 times, and drying in a 100 ℃ oven for 12h;
(1-2) dissolving boric acid in pure methanol to prepare a precursor solution, wherein the mass ratio of the boric acid to the methanol is 1:3, immersing the short carbon fibers obtained in the step (1-1) into the precursor solution, ultrasonically stirring for 60min, separating the treated short carbon fibers from the solution, and putting the solution into a drying oven at 100 ℃ until the short carbon fibers are completely dried;
(1-3) placing the boronated short carbon fiber obtained in step (1-2) into a zirconia crucible and installing in a heating pipe; introducing ammonia gas at a speed of 50cc/min under the condition of nitrogen, heating to 1400 ℃, continuing for 60min, stopping flowing of the ammonia gas after 2h, and cooling under the atmosphere of nitrogen to obtain boron nitride modified short carbon fibers;
(2) Adding the boron nitride modified short carbon fiber, the fused quartz powder and the pure water prepared in the step (1) into a roller ball mill for mixed ball milling to obtain slurry; the adding amount of the boron nitride modified short carbon fiber is 20wt% of the slurry; the addition amount of the fused quartz powder is 70wt% of the slurry; the addition amount of the pure water is 10wt% of the slurry; the rotating speed of the ball mill is 30r/min, and the ball milling time is 24h;
(3) Adding the mixed slurry obtained in the step (2) into a gypsum mold for molding;
(4) And (3) placing the biscuit molded in the step (3) into an oven with the temperature of 120 ℃ to be dried for 12 hours, finally placing the biscuit into a muffle furnace, heating to 1250 ℃ from room temperature at the speed of 15 ℃/min under the air condition, and preserving heat for 3 hours to obtain boron nitride modified short carbon fiber reinforced fused silica ceramic, and respectively testing the dielectric constant, the thermal conductivity and the bending strength of the ceramic, wherein the testing standard or method and the obtained performance parameters are shown in the following table 3.
TABLE 3 Performance test results of boron nitride modified short carbon fiber reinforced fused silica ceramics
Performance of | Test standard/method | Performance parameters |
Dielectric constant | Short circuit waveguide method | 3.5 |
Thermal conductivity (W/m.K) | Laser pulse method | <0.61 |
Flexural Strength (MPa) | GB/T 6569-2006 | 155 |
As can be seen from tables 1 to 3, the boron nitride modified short carbon fiber reinforced fused quartz ceramic prepared by the invention has high bending strength which reaches 153MPa at the lowest; the dielectric constant is less than or equal to 3.5, and the dielectric performance is not reduced; the thermal conductivity is also substantially unchanged. Therefore, the boron nitride modified short carbon fiber reinforced fused quartz ceramic prepared by the invention has high strength, low thermal conductivity and good dielectric property, and is an ideal radome material.
Claims (7)
1. The preparation method of the boron nitride modified short carbon fiber reinforced fused quartz ceramic is characterized by comprising the following steps of:
(1) Boron nitride modified short carbon fibers;
firstly, chopping carbon fibers to obtain short carbon fibers, then placing the short carbon fibers in acetone for soaking, then washing with distilled water and drying;
dissolving boric acid in pure methanol to obtain a precursor solution, completely immersing the short carbon fiber obtained in the step (1-1) in the precursor solution, ultrasonically stirring, separating the treated short carbon fiber from the solution, and drying in an oven;
(1-3) placing the boronized short carbon fibers obtained in the step (1-2) into a zirconia crucible, installing the crucible in a heating pipe, and introducing ammonia gas under the condition of nitrogen gas for heating to obtain boron nitride modified short carbon fibers;
(2) Adding the boron nitride modified short carbon fiber, fused quartz powder and pure water obtained in the step (1) into a ball mill for mixing and ball milling to obtain slurry;
(3) Adding the slurry mixed in the step (2) into a gypsum mold to form a biscuit;
(4) And (3) placing the biscuit obtained in the step (3) into an oven for drying, and finally placing the biscuit into a muffle furnace for sintering to obtain the boron nitride modified short carbon fiber reinforced fused quartz ceramic.
2. The method for preparing a boron nitride modified short carbon fiber reinforced fused silica ceramic according to claim 1, wherein in the step (2), the addition amount of the boron nitride modified short carbon fiber is 5wt.% to 20wt.% of the slurry; the addition amount of the fused quartz powder is 70-80 wt.% of the slurry; the addition amount of the pure water is 10wt.% to 15wt.% of the slurry.
3. The method for preparing boron nitride modified short carbon fiber reinforced fused silica ceramic according to claim 1 or 2, wherein in the step (2), the rotation speed of the ball mill is 15-30r/min, and the ball milling time is 12-24h.
4. The method for preparing boron nitride modified short carbon fiber reinforced fused silica ceramic according to claim 1 or 2, wherein in the step (4), the drying environment of the green body is: drying in an oven at 80-120 ℃ for 12-24 h; the specific system of sintering is as follows: and (3) placing the dried biscuit in a muffle furnace, heating to 1150-1250 ℃ from room temperature at a speed of 15 ℃/min under the air condition, and preserving heat for 3-5 hours to obtain the boron nitride modified short carbon fiber reinforced fused silica ceramic.
5. The method for preparing boron nitride modified short carbon fiber reinforced fused silica ceramic according to claim 1 or 2, wherein in the step (1-3), the specific process of introducing ammonia gas for heating is as follows: introducing ammonia gas at a speed of 10-50cc/min under the nitrogen condition, heating to 1400 ℃, preserving heat for 60-120min, stopping flowing of the ammonia gas after 1-2h, and cooling under the nitrogen atmosphere to obtain the boron nitride modified short carbon fiber.
6. The method for preparing a boron nitride modified short carbon fiber reinforced fused silica ceramic according to claim 1 or 2, wherein in the step (1-2), the mass ratio between boric acid and methanol is 1 (1-3); stirring by ultrasonic for 40-60min; the drying temperature of the oven is 60-100 ℃.
7. The method for producing a boron nitride modified short carbon fiber reinforced fused silica ceramic according to claim 1 or 2, wherein in the step (1-1), the short carbon fiber has a length of 3 to 5cm; soaking short carbon fiber in acetone for 12-24 hr, washing with distilled water for 3-5 times, and drying in oven at 60-100deg.C for 12-24 hr.
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